CN109585917A - A kind of polymer dielectric and preparation method thereof and the battery including the polymer dielectric - Google Patents
A kind of polymer dielectric and preparation method thereof and the battery including the polymer dielectric Download PDFInfo
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- CN109585917A CN109585917A CN201811507140.2A CN201811507140A CN109585917A CN 109585917 A CN109585917 A CN 109585917A CN 201811507140 A CN201811507140 A CN 201811507140A CN 109585917 A CN109585917 A CN 109585917A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0082—Organic polymers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to polymer dielectric preparation technical fields, and in particular to a kind of polymer dielectric and preparation method thereof and the battery including the polymer dielectric；The polymer dielectric includes polymeric matrix, organic solvent, inorganic filler, the first solution and the second solution；The polymeric matrix and inorganic filler dispersion are in organic solvent；The inorganic filler is one of modified calcium-base montmorillonite, modified nano calcium carbonate, nano-nickel oxide or a variety of；The preparation method of modified calcium-base montmorillonite is to realize calcium-base montmorillonite and cetyl trimethylammonium bromide ball milling modification；The present invention provides a kind of polymer dielectric and preparation method thereof and including the battery of the polymer dielectric, polymer dielectric prepared by the present invention has higher thermodynamic stability, ionic conductivity, better mechanical strength and electrochemical stability.
Description
Technical field
The present invention relates to polymer dielectric preparation technical fields, and in particular to a kind of polymer dielectric and its preparation side
Method and battery including the polymer dielectric.
Background technique
With the development of world economy, demand of the people to the energy is increasing, it is desirable that and it is also higher and higher, it has become complete
The tracking hot spot and world trends of ball.Lithium ion battery is a Main way of new energy development, and lithium ion battery is not only wide
It is general to be applied in daily life electric appliance such as mobile phone, notebook, tablet computer, also in electric car, hybrid vehicle
It makes first appearance.Existing more common inorganic material generally has oxide material, ferroelectric substance, lithium-containing compound, molecular sieve, consolidates
This few major class material of body acid, doping way generally use direct feeding method, i.e., inorganic material are added directly into polymeric matrix
In, it is dispersed inorganic particulate in polymeric matrix by mechanical stirring or supersonic oscillations.
If Chinese Patent Application No. is that CN201210382299.2 discloses a kind of all-solid-state nano composite polymer electrolysis
Surface-functionalized graphene, dissociable lithium salts and polymeric matrix are mixed and are dissolved in organic solvent by the preparation method of matter, are led to
It crosses ultrasonication and mechanical stirring obtains sol form compound；It is cast in polytetrafluoroethylene (PTFE) template, in a vacuum drying oven
It is dry, obtain dielectric film.But its prepare Room-temperature-conductivity of Polymer Electrolyte it is lower, and lithium ion transference number also compared with
It is low, desirable can not be reached, while the mechanical property of polymer dielectric, electrochemical stability and thermal stability also do not reach
To desirable, for this purpose, for a kind of polymer dielectric and preparation method thereof and including the battery of the polymer dielectric, I
Need to provide a kind of new approaches.
Summary of the invention
In view of the deficiencies of the prior art, poly- the present invention provides a kind of polymer dielectric and preparation method thereof and including this
The battery of polymer electrolyte, polymer dielectric prepared by the present invention have higher thermodynamic stability, ionic conductivity, more
Good mechanical strength and electrochemical stability.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of polymer dielectric, the polymer dielectric include polymeric matrix, organic solvent, inorganic filler, the first solution
With the second solution；The polymeric matrix and inorganic filler dispersion are in organic solvent；The inorganic filler is modified calcium-base illiteracy
One of de- soil, modified nano calcium carbonate, nano-nickel oxide are a variety of；
The preparation method of the modified calcium-base montmorillonite is by calcium-base montmorillonite and cetyl trimethylammonium bromide ball milling modification
It realizes；
The preparation method of the modified nano calcium carbonate is will to be modified realization to nanometer calcium carbonate using titanate coupling agent
's.
Preferably, the polymeric matrix is polyethylene glycol oxide, polymethyl methacrylate, polyvinyl chloride, polyvinylidene fluoride
One of alkene, polyacrylonitrile are a variety of.
Preferably, the organic solvent is n,N-Dimethylformamide, n,N-dimethylacetamide, acetone, chloroform, acetonitrile
One of or it is a variety of.
Preferably, first solution is LiPF6、LiBF4、LiAsF6、LiClO4、LiCF3SO3、LiN(CF3SO2)2In
One or more dispersion liquids.
More preferably, first solution is LiPF6Dispersion liquid, it is 1:2:1 that high-purity LiF, which is dispersed in mass ratio,
In the mixed solution of DMC, DEC, EC, stir into uniform suspension, 20-40 degrees Celsius at a temperature of be passed through PF5, control lithium
The molar content of ion is 0.1-1mol/L, up to LiPF6Dispersion liquid.
Preferably, second solution is ethylene carbonate, in propene carbonate, diethyl carbonate, methyl ethyl carbonate
It is one or more.
A kind of polymer dielectric, preparation method includes the following steps:
S1, above-mentioned polymeric matrix, inorganic filler are added into organic solvent under stirring conditions, form homogeneous transparent
This suspension is cast in substrate drying, obtains polymer film by suspension after decompression standing removes bubble removing；
S2, above-mentioned polymer film is placed in scattered first solution, control electrophoretic deposition voltage, electrophoretic deposition electric current and
The electrophoretic deposition time obtains dielectric film after 70-90 DEG C of vacuum drying；
S3, in vacuum glove box, by dielectric film obtained above be placed in the second solution impregnate 1-3h to get electrostrictive polymer
Xie Zhi.
Preferably, the electrophoretic deposition voltage in the S2 is 15-25V；Electrophoretic deposition electric current is 20-80mA；Electrophoretic deposition
Time is 30-50min.
Preferably, which includes anode, cathode and polymer dielectric, and the polymer dielectric is located at just
Between pole and cathode.
Since the present invention mainly improves the polymer dielectric in polymer battery, to formation electrostrictive polymer
There is no particular limitation for anode, cathode and the battery case in pond and their structural relation, and the anode and cathode can be this
The well known various anodes and cathode in polymer battery of field technology.
There is no particular limitation for the preparation method of polymer battery by the present invention, the electrostrictive polymer that will can be prepared in advance
Solution matter film is adhered to a surface of positive plate and negative electrode tab, then keeps the surface of two polymer dielectric films opposite
In the case of by the positive plate for being stained with polymer dielectric film and the negative electrode tab for being stained with polymer dielectric film be stacked or winding,
Pole piece is formed, then pole piece is placed in battery case, by sealing, chemical conversion, sealing, packaging；It can also be poly- by preparation
The mixed solution of polymer electrolyte be coated in battery anode slice and negative electrode tab a surface, then by removal solvent to
Positive plate and negative electrode tab surface form polymer dielectric film, later in the feelings for keeping the surface of two polymer dielectric films opposite
The positive plate including polymer dielectric film and the negative electrode tab including polymer dielectric film are stacked or are wound under condition, is formed
Then pole piece is placed in battery case by pole piece, by sealing, chemical conversion, sealing, packaging；It can also be by the polymerization of preparation
The mixed solution of object electrolyte is coated in a surface of battery anode slice and negative electrode tab, then by removal solvent to just
Pole piece and negative electrode tab surface form polymer dielectric film, later in the side for the positive plate for being stained with polymer dielectric and viscous
The polymer dielectric prepared is added between the side of negative electrode tab with polymer dielectric and winds sealing, is then passed through
Chemical conversion, sealing, packaging, wherein the polymer dielectric of the addition not only includes the polymer electrolytic prepared in text
The use of matter, other polymer dielectrics and battery separator is also within protection scope, and the operation of the sealing and chemical conversion is
Known to those skilled in the art, no longer chela is stated herein.
The invention has the following advantages: the present invention on the basis of polymeric matrix, is added to nano-scale particle
Inorganic filler is modified, and has obtained the polymer film of function admirable, due to nanometer particle have unique small-size effect,
Quantum size effect and skin effect, so the polymer film has the fabulous microcellular structure being cross-linked with each other, splendid imbibition
Performance is dispersed in the first solution, and after electrophoretic deposition, the mechanical strength of polymer film is obviously improved, and is continued molten second
It is impregnated in liquid, after forming electrolyte, test indicate that polymer dielectric prepared by the present invention has higher Thermodynamically stable
Property, ionic conductivity, better mechanical strength and electrochemical stability；And polymer dielectric provided by the present invention has
Cross-linked network can balance all directions to Li+Active force, thereby reduce Li+Dissociation energy, and then improve lithium from
The transport number of son, and then make polymer electrolyte battery ionic conductivity with higher and mechanical strength；And the present invention
Provided polymer dielectric is due to using modified calcium-base montmorillonite, modified nano calcium carbonate, nano-nickel oxide as inorganic
Filler improves the structure of polymeric matrix as dopant, enhances the noncrystalline phase of polymeric matrix, and then make to gather
The room-temperature conductivity and lithium ion transference number of polymer electrolyte have obtained significant raising, while also to the boundary of polymer dielectric
Face stability is improved；Detection is carried out by the performance to the polymer dielectric prepared in the embodiment of the present invention to show
Its room-temperature conductivity of polymer dielectric provided by the present invention is up to 7.8 × 10-4S/cm, lithium ion transference number are up to 0.68,
And the room-temperature conductivity of the polymer dielectric in documents is only 6.7 × 10-4S/cm, lithium ion transference number are only 0.62.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A kind of polymer dielectric, the polymer dielectric include polymeric matrix, organic solvent, inorganic filler, the first solution
With the second solution；Polymeric matrix and inorganic filler dispersion are in organic solvent；Inorganic filler is modified calcium-base montmorillonite, modification
Two kinds of mixtures of nanometer calcium carbonate；
Polymeric matrix is two kinds of mixtures of polyethylene glycol oxide, polymethyl methacrylate.
Organic solvent is n,N-Dimethylformamide.
First solution is LiPF6Dispersion liquid.
Second solution is ethylene carbonate.
A kind of polymer dielectric, preparation method includes the following steps:
S1, by above-mentioned suitable polyethylene glycol oxide, polymethyl methacrylate, modified calcium-base montmorillonite, modified nano calcium carbonate
It is added under stirring conditions according to the mass ratio of 13:1.5:1.5:1.5 into 100 parts of n,N-Dimethylformamide, is formed
This suspension is cast in substrate drying, obtains polymer by the suspension of homogeneous transparent after decompression standing removes bubble removing
Film；
S2, above-mentioned polymer film is placed in scattered first solution, control electrophoretic deposition voltage, electrophoretic deposition electric current and
The electrophoretic deposition time obtains dielectric film after 80 DEG C of vacuum drying；
S3, in vacuum glove box, by dielectric film obtained above be placed in the second solution impregnate 2.5h to get electrostrictive polymer
Xie Zhi.
Electrophoretic deposition voltage in S2 is 15V；Electrophoretic deposition electric current is 20mA；The electrophoretic deposition time is 30min.
Embodiment 2:
A kind of polymer dielectric, the polymer dielectric include polymeric matrix, organic solvent, inorganic filler, the first solution
With the second solution；Polymeric matrix and inorganic filler dispersion are in organic solvent；Inorganic filler is modified calcium-base montmorillonite, nanometer
The mixture of nickel oxide；
Polymeric matrix is two kinds of mixtures of polyethylene glycol oxide, polyvinyl chloride.
Preferably, the organic solvent is n,N-dimethylacetamide.
First solution is LiBF4Dispersion liquid.
Second solution is ethylene carbonate.
A kind of polymer dielectric, preparation method includes the following steps:
S1, by above-mentioned polyethylene glycol oxide, polyvinyl chloride, modified calcium-base montmorillonite, nano-manganese dioxide according to 13:1.5:1.5:
1.5 mass ratio is added into organic solvent under stirring conditions, forms the suspension of homogeneous transparent, stands removal through decompression
After bubble, this suspension is cast drying in substrate, obtains polymer film；
S2, above-mentioned polymer film is placed in scattered first solution, control electrophoretic deposition voltage, electrophoretic deposition electric current and
The electrophoretic deposition time obtains dielectric film after 80 DEG C of vacuum drying；
S3, in vacuum glove box, by dielectric film obtained above be placed in the second solution impregnate 2.5h to get electrostrictive polymer
Xie Zhi.
Electrophoretic deposition voltage in S2 is 20V；Electrophoretic deposition electric current is 40mA；The electrophoretic deposition time is 30min.
Embodiment 3:
A kind of polymer dielectric, the polymer dielectric include polymeric matrix, organic solvent, inorganic filler, the first solution
With the second solution；Polymeric matrix and inorganic filler dispersion are in organic solvent；Inorganic filler is modified calcium-base montmorillonite, nanometer
Two kinds of mixtures in nickel oxide；
Polymeric matrix is two kinds of mixtures of polyethylene glycol oxide, Kynoar.
Organic solvent is acetone.
First solution is LiAsF6Dispersion liquid.
Second solution is diethyl carbonate.
A kind of polymer dielectric, preparation method includes the following steps:
S1, by above-mentioned polyethylene glycol oxide, Kynoar, modified calcium-base montmorillonite, nano-nickel oxide according to 13:1.5:1.5:
1.5 mass ratio is added into organic solvent under stirring conditions, forms the suspension of homogeneous transparent, stands removal through decompression
After bubble, this suspension is cast drying in substrate, obtains polymer film；
S2, above-mentioned polymer film is placed in scattered first solution, control electrophoretic deposition voltage, electrophoretic deposition electric current and
The electrophoretic deposition time obtains dielectric film after 80 DEG C of vacuum drying；
S3, in vacuum glove box, by dielectric film obtained above be placed in the second solution impregnate 2.5h to get electrostrictive polymer
Xie Zhi.
Electrophoretic deposition voltage in S2 is 25V；Electrophoretic deposition electric current is 60mA；The electrophoretic deposition time is 30min.
Embodiment 4:
A kind of polymer dielectric, the polymer dielectric include polymeric matrix, organic solvent, inorganic filler, the first solution
With the second solution；Polymeric matrix and inorganic filler dispersion are in organic solvent；Inorganic filler is modified calcium-base montmorillonite, nanometer
Two kinds of mixtures of nickel oxide；
Polymeric matrix is two kinds of mixtures of polyethylene glycol oxide, polyacrylonitrile.
Preferably, the organic solvent is chloroform.
First solution is LiClO4Dispersion liquid.
Second solution is carbon methyl ethyl carbonate.
A kind of polymer dielectric, preparation method includes the following steps:
S1, by above-mentioned polyethylene glycol oxide, polyacrylonitrile, modified calcium-base montmorillonite, nano-nickel oxide according to 13:1.5:1.5:1.5
Mass ratio be added under stirring conditions into organic solvent, form the suspension of homogeneous transparent, through decompression stand go degasification
After bubble, this suspension is cast drying in substrate, obtains polymer film；
S2, above-mentioned polymer film is placed in scattered first solution, control electrophoretic deposition voltage, electrophoretic deposition electric current and
The electrophoretic deposition time obtains dielectric film after 80 DEG C of vacuum drying；
S3, in vacuum glove box, by dielectric film obtained above be placed in the second solution impregnate 2.5h to get electrostrictive polymer
Xie Zhi.
Electrophoretic deposition voltage in S2 is 25V；Electrophoretic deposition electric current is 60mA；The electrophoretic deposition time is 30min.
Embodiment 5:
A kind of polymer dielectric, the polymer dielectric include polymeric matrix, organic solvent, inorganic filler, the first solution
With the second solution；Polymeric matrix and inorganic filler dispersion are in organic solvent；Inorganic filler is modified calcium-base montmorillonite, modification
The mixture of nanometer calcium carbonate, modified Nano nickel oxide；
Modified Nano nickel oxide forms urea, Nickel dichloride hexahydrate, the sodium citrate dispersion that molar ratio is 4:1:4 in ethanol
Mixed liquor will carry out thermal response after mixed liquor sealing, by product washing, drying, then with molar ratio 1:100 under 200 °C
Amount by product be added 1- butyl -3- methyl imidazolium tetrafluoroborate ionic liquid in, carried out again under 200 °C after sealing
Heat treatment is ground under an argon atmosphere with 2 °C/min temperature programming to natural cooling after 500 °C after product washing, drying
It grinds to obtain the final product.
Polymeric matrix is two kinds of mixtures of polyethylene glycol oxide, polyacrylonitrile.
Preferably, the organic solvent is acetonitrile.
First solution is LiPF6Dispersion liquid.
Second solution is ethylene carbonate.
A kind of polymer dielectric, preparation method includes the following steps:
S1, by above-mentioned polyethylene glycol oxide, polyacrylonitrile, modified calcium-base montmorillonite, modified nano calcium carbonate according to 13:1.5:1.5:
1.5 mass ratio is added into organic solvent under stirring conditions, forms the suspension of homogeneous transparent, stands removal through decompression
After bubble, this suspension is cast drying in substrate, obtains polymer film；
S2, above-mentioned polymer film is placed in scattered first solution, control electrophoretic deposition voltage, electrophoretic deposition electric current and
The electrophoretic deposition time obtains dielectric film after 80 DEG C of vacuum drying；
S3, in vacuum glove box, by dielectric film obtained above be placed in the second solution impregnate 2.5h to get electrostrictive polymer
Xie Zhi.
Electrophoretic deposition voltage in S2 is 20V；Electrophoretic deposition electric current is 40mA；The electrophoretic deposition time is 30min.
Electrolyte prepared by above-described embodiment 1-5 is assembled into electrolytic cell, performance detection is carried out to it, detection data is such as
Shown in following table:
。
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (8)
1. a kind of polymer dielectric, it is characterised in that: the polymer dielectric includes polymeric matrix, organic solvent, inorganic
Filler, the first solution and the second solution；The polymeric matrix and inorganic filler dispersion are in organic solvent；The inorganic filler
For one of modified calcium-base montmorillonite, modified nano calcium carbonate, nano-nickel oxide or a variety of；
The preparation method of the modified calcium-base montmorillonite is by calcium-base montmorillonite and cetyl trimethylammonium bromide ball milling modification
It realizes；
The preparation method of the modified nano calcium carbonate is will to be modified realization to nanometer calcium carbonate using titanate coupling agent
's.
2. a kind of polymer dielectric according to claim 1, it is characterised in that: the polymeric matrix is polyoxyethylene
One of alkene, polymethyl methacrylate, polyvinyl chloride, Kynoar, polyacrylonitrile are a variety of.
3. a kind of polymer dielectric according to claim 1, it is characterised in that: the organic solvent is N, N- dimethyl
One of formamide, n,N-dimethylacetamide, acetone, chloroform, acetonitrile are a variety of.
4. a kind of polymer dielectric according to claim 1, it is characterised in that: first solution is LiPF6、
LiBF4、LiAsF6、LiClO4、LiCF3SO3、LiN(CF3SO2)2One of or a variety of dispersion liquids.
5. a kind of polymer dielectric according to claim 1, it is characterised in that: second solution is ethylene carbonate
One of ester, propene carbonate, diethyl carbonate, methyl ethyl carbonate are a variety of.
6. a kind of method for preparing polymer electrolytes described in claim 1, which is characterized in that preparation method includes following
Step:
S1, above-mentioned polymeric matrix, inorganic filler are added into organic solvent under stirring conditions, form homogeneous transparent
This suspension is cast in substrate drying, obtains polymer film by suspension after decompression standing removes bubble removing；
S2, above-mentioned polymer film is placed in scattered first solution, control electrophoretic deposition voltage, electrophoretic deposition electric current and
The electrophoretic deposition time obtains dielectric film after 70-90 DEG C of vacuum drying；
S3, in vacuum glove box, by dielectric film obtained above be placed in the second solution impregnate 1-3h to get electrostrictive polymer
Xie Zhi.
7. a kind of method for preparing polymer electrolytes according to claim 6, it is characterised in that: the electrophoresis in the S2
Deposition voltage is 15-25V；Electrophoretic deposition electric current is 20-80mA；The electrophoretic deposition time is 30-50min.
8. a kind of battery using polymer dielectric as described in claim 1, it is characterised in that: the battery include anode,
Cathode and polymer dielectric, the polymer dielectric are located between anode and cathode.
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